 
data_cuhg032 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 H0 Br8 Cu Hg3 N4 O5' 
_chemical_formula_weight          1584.75 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Hg'  'Hg'  -2.3894   9.2266 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 
_cell_length_a                    7.976(4) 
_cell_length_b                    10.463(4) 
_cell_length_c                    10.862(3) 
_cell_angle_alpha                 75.43(3) 
_cell_angle_beta                  78.76(4) 
_cell_angle_gamma                 68.30(5) 
_cell_volume                      809.9(6) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.249 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              689 
_exptl_absorpt_coefficient_mu     24.714 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2837 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0437 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.03 
_diffrn_reflns_theta_max          24.98 
_reflns_number_total              2837 
_reflns_number_gt                 2406 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+20.4492P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.04(4) 
_refine_ls_number_reflns          2837 
_refine_ls_number_parameters      193 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0884 
_refine_ls_R_factor_gt            0.0713 
_refine_ls_wR_factor_ref          0.2165 
_refine_ls_wR_factor_gt           0.1925 
_refine_ls_goodness_of_fit_ref    1.108 
_refine_ls_restrained_S_all       1.107 
_refine_ls_shift/su_max           0.221 
_refine_ls_shift/su_mean          0.025 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Hg1 Hg 0.8368(3) 0.8848(3) 0.9633(3) 0.0334(4) Uani 1 d . . . 
Hg2 Hg 0.8608(2) 1.19599(17) 0.57256(16) 0.0421(6) Uani 1 d . . . 
Hg3 Hg 0.8180(2) 1.56317(18) 0.35352(17) 0.0424(6) Uani 1 d . . . 
Br1 Br 0.8870(8) 1.5580(5) 0.1191(6) 0.0358(12) Uani 1 d . . . 
Br2 Br 0.5853(8) 1.4127(6) 0.4450(6) 0.0410(14) Uani 1 d . . . 
Br3 Br 0.7767(8) 1.2084(6) 0.8060(6) 0.0438(15) Uani 1 d . . . 
Br4 Br 0.7665(9) 1.7170(6) 0.5074(6) 0.0484(16) Uani 1 d . . . 
Br5 Br 0.6929(7) 0.8730(6) 0.7930(5) 0.0402(14) Uani 1 d . . . 
Br6 Br 0.9710(8) 0.8921(6) 1.1418(6) 0.0423(15) Uani 1 d . . . 
Br7 Br 1.0961(7) 1.3392(6) 0.4736(6) 0.0385(13) Uani 1 d . . . 
Br8 Br 0.9360(8) 1.0240(6) 0.4298(6) 0.0422(14) Uani 1 d . . . 
Cu1 Cu 0.3662(10) 0.8758(7) 0.4669(7) 0.0289(15) Uani 1 d . . . 
C11 C 0.233(6) 0.838(5) 0.729(5) 0.025(10) Uiso 1 d . . . 
O11 O 0.308(4) 0.920(3) 0.637(3) 0.034(7) Uiso 1 d . . . 
O12 O 0.191(4) 0.851(3) 0.832(3) 0.019(6) Uiso 1 d . . . 
C12 C 0.193(5) 0.726(4) 0.673(4) 0.027(8) Uiso 1 d . . . 
N11 N 0.285(5) 0.704(4) 0.554(3) 0.025(8) Uiso 1 d . . . 
C13 C 0.242(5) 0.584(4) 0.778(4) 0.027(9) Uiso 1 d . . . 
C14 C 0.206(5) 0.469(4) 0.734(4) 0.027(8) Uiso 1 d . . . 
C15 C 0.235(5) 0.333(4) 0.842(4) 0.017(7) Uiso 1 d . . . 
C16 C 0.230(8) 0.213(6) 0.791(6) 0.052(13) Uiso 1 d . . . 
N12 N 0.226(5) 0.096(4) 0.898(4) 0.034(10) Uiso 1 d . . . 
C21 C 0.434(6) 0.933(4) 0.210(4) 0.021(9) Uiso 1 d . . . 
O21 O 0.426(3) 0.829(2) 0.299(2) 0.014(5) Uiso 1 d . . . 
O22 O 0.464(3) 0.930(3) 0.087(3) 0.017(6) Uiso 1 d . . . 
C22 C 0.402(5) 1.075(4) 0.243(4) 0.025(7) Uiso 1 d . . . 
N21 N 0.432(4) 1.042(3) 0.388(3) 0.022(7) Uiso 1 d . . . 
C23 C 0.498(5) 1.166(4) 0.158(4) 0.025(8) Uiso 1 d . . . 
C24 C 0.412(6) 1.320(4) 0.184(4) 0.032(9) Uiso 1 d . . . 
C25 C 0.488(6) 1.423(5) 0.089(4) 0.031(10) Uiso 1 d . . . 
C26 C 0.395(5) 1.567(4) 0.123(4) 0.022(8) Uiso 1 d . . . 
N22 N 0.444(5) 1.682(4) 0.028(4) 0.026(8) Uiso 1 d . . . 
O02 O 0.708(4) 0.538(3) 0.825(3) 0.042(7) Uiso 1 d . . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Hg1 0.0357(7) 0.0426(7) 0.0277(6) -0.0136(5) 0.0049(5) -0.0197(6) 
Hg2 0.0517(13) 0.0490(14) 0.0296(14) -0.0170(10) 0.0026(10) -0.0193(11) 
Hg3 0.0534(14) 0.0481(13) 0.0310(14) -0.0130(10) 0.0033(11) -0.0236(10) 
Br1 0.049(3) 0.036(3) 0.025(3) 0.003(2) 0.001(2) -0.025(2) 
Br2 0.037(3) 0.040(3) 0.044(4) -0.002(2) -0.005(2) -0.014(2) 
Br3 0.057(3) 0.047(3) 0.025(3) -0.012(2) 0.012(3) -0.019(3) 
Br4 0.066(4) 0.041(3) 0.042(3) -0.019(2) -0.013(3) -0.011(2) 
Br5 0.042(3) 0.058(3) 0.028(3) -0.009(3) 0.008(2) -0.031(2) 
Br6 0.055(3) 0.042(3) 0.033(3) -0.019(3) -0.008(3) -0.011(2) 
Br7 0.034(3) 0.041(3) 0.038(3) -0.007(2) 0.004(2) -0.014(2) 
Br8 0.060(3) 0.035(3) 0.037(3) -0.013(2) 0.006(2) -0.023(2) 
Cu1 0.058(4) 0.0191(18) 0.0113(16) 0.0006(14) 0.012(2) -0.025(2) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Hg1 Br5 2.409(7) . ? 
Hg1 Br6 2.420(6) . ? 
Hg2 Br8 2.499(6) . ? 
Hg2 Br3 2.517(6) . ? 
Hg2 Br7 2.721(7) . ? 
Hg2 Br2 2.795(6) . ? 
Hg3 Br4 2.480(6) . ? 
Hg3 Br1 2.508(6) . ? 
Hg3 Br2 2.751(7) . ? 
Hg3 Br7 2.803(6) . ? 
Cu1 O11 1.94(3) . ? 
Cu1 O21 1.94(2) . ? 
Cu1 N11 2.07(4) . ? 
Cu1 N21 1.94(3) . ? 
C11 O12 1.14(5) . ? 
C11 O11 1.35(6) . ? 
C11 C12 1.59(6) . ? 
C12 N11 1.39(5) . ? 
C12 C13 1.60(5) . ? 
C13 C14 1.53(5) . ? 
C14 C15 1.58(5) . ? 
C15 C16 1.51(6) . ? 
C16 N12 1.46(7) . ? 
C21 O21 1.27(5) . ? 
C21 O22 1.32(5) . ? 
C21 C22 1.53(5) . ? 
C22 N21 1.56(5) . ? 
C22 C23 1.47(5) . ? 
C23 C24 1.58(5) . ? 
C24 C25 1.50(6) . ? 
C25 C26 1.52(5) . ? 
C26 N22 1.50(5) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
Br5 Hg1 Br6 177.2(3) . . ? 
Br8 Hg2 Br3 139.6(2) . . ? 
Br8 Hg2 Br7 103.7(2) . . ? 
Br3 Hg2 Br7 107.7(2) . . ? 
Br8 Hg2 Br2 98.6(2) . . ? 
Br3 Hg2 Br2 105.8(2) . . ? 
Br7 Hg2 Br2 90.5(2) . . ? 
Br4 Hg3 Br1 142.0(2) . . ? 
Br4 Hg3 Br2 106.3(2) . . ? 
Br1 Hg3 Br2 104.5(2) . . ? 
Br4 Hg3 Br7 95.5(2) . . ? 
Br1 Hg3 Br7 106.30(19) . . ? 
Br2 Hg3 Br7 89.70(19) . . ? 
Hg3 Br2 Hg2 89.65(19) . . ? 
Hg2 Br7 Hg3 90.09(18) . . ? 
O11 Cu1 O21 179.2(13) . . ? 
O11 Cu1 N11 84.8(13) . . ? 
O21 Cu1 N11 94.6(12) . . ? 
O11 Cu1 N21 94.0(14) . . ? 
O21 Cu1 N21 86.6(12) . . ? 
N11 Cu1 N21 177.6(15) . . ? 
O12 C11 O11 124(4) . . ? 
O12 C11 C12 123(4) . . ? 
O11 C11 C12 112(4) . . ? 
C11 O11 Cu1 116(3) . . ? 
N11 C12 C13 111(3) . . ? 
N11 C12 C11 115(4) . . ? 
C13 C12 C11 106(3) . . ? 
C12 N11 Cu1 108(2) . . ? 
C12 C13 C14 110(3) . . ? 
C15 C14 C13 111(3) . . ? 
C14 C15 C16 111(4) . . ? 
N12 C16 C15 110(4) . . ? 
O21 C21 O22 124(4) . . ? 
O21 C21 C22 120(4) . . ? 
O22 C21 C22 116(4) . . ? 
C21 O21 Cu1 112(2) . . ? 
N21 C22 C23 115(3) . . ? 
N21 C22 C21 106(3) . . ? 
C23 C22 C21 118(3) . . ? 
C22 N21 Cu1 107(2) . . ? 
C22 C23 C24 111(3) . . ? 
C23 C24 C25 113(4) . . ? 
C26 C25 C24 109(4) . . ? 
C25 C26 N22 114(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              24.98 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    3.090 
_refine_diff_density_min   -5.237 
_refine_diff_density_rms    0.503 
